反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To N-[6-(1-tert-butyloxycarbonylpiperidin-4-yl)-5-methylpyridin-3-yl]-5-methyl-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxamide (7.0 g) were added dichloromethane (128 ml) and trifluoroacetic acid (26 ml), stirred at room temperature for 2 hours, and then to the reaction solution was added 4 N aqueous solution of sodium hydroxide under ice-cooling. The precipitated solid was washed with n-hexane and water, the obtained solid was dissolved in chloroform, water was added thereto, extracted with chloroform and ethyl acetate, dried over anhydrous sodium sulfate, and then the solvent was evaporated in vacuo. The precipitated solid was washed with ethyl acetate to give the titled compound (5.39 g) as a white solid.
WORKUP
后处理
- temperaturecooling
- washThe precipitated solid was washed with n-hexane and water
- dissolutionthe obtained solid was dissolved in chloroform
- additionwater was added
- extractionextracted with chloroform and ethyl acetate
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent was evaporated in vacuo
- washThe precipitated solid was washed with ethyl acetate